Water → HCID 89526079, compound

Participants

Reaction Steps

To a suspension of NaH (567 mg, 14.2 mmol, 60%) in DMSO (30 mL) was added dropwise a solution of Example 85D (1.2 g, 6.45 mmol) in THF (5 mL) at room temperature and then the mixture was stirred for 30 minutes, followed by the addition of a solution of 1,3-dibromopropane (1.4 g, 7.10 mmol) in THF (5 mL) at room temperature. The mixture was stirred for additional 2 hours. After addition of water (30 mL) carefully, the resulting mixture was extracted with EtOAc (30 mL×2). The combined organic layers were washed with water (30 mL) and brine (30 mL), dried over Na2SO4, filtered, and concentrated to provide the title compound (1.45 g, 6.45 mmol, yield 100%) as a oil. The crude product was used in the next step without further purification. LC-MS: m/z 227.2 (M+H)+.

Provenance & Evidence